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After 45 min at rt, the orange solution was cooled to 0 °C, and a solution of bromo alcohol 10a (68 mg, 0.15 mmol) in dry THF (2 mL) was cautiously added.
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The corresponding mixture was stirred for 15 min, and then a solution of 11-bromo-1-undecanol (7) (2.512 g, 10 mmol) in CH2Cl2 (10 mL) was added dropwise over 5 min.
To a solution of 12-bromo dodecane-1-ol (12.6 g, 47.4 mmol) indimethyl sulfoxide (200 ml) was added sodium azide (15.4 g, 237 mmol), with the solution stirred at 80°C for 1 week.
To a solution of 10-bromo-2-ethyldecane acid (4.29 g) in ethanol (150 ml), an aqueous solution of trimethylamine (Fluka, 45 50 %, 30 ml) was added.
3-Bromo-4-methylphenyl benzoate (19 a): Benzoyl chloride (1.65 g, 11.7 mmol) was added dropwise to a solution of 3-bromo-4-methylphenol (2.00 g, 10.7 mmol) and pyridine (3 mL) in CH2Cl2 (20 mL).
A solution of 1-bromo-2 tert-butoxyethene (8.32 g, 0.047 mol) in THF (45 mL) was then added dropwise to the solution at –70 °C, and the resulting mixture was warmed to room temp.
The staining reaction was initiated by adding a solution of 5-bromo-4-chloro-3-indolyl-phosphate (BCIP /nitroblue tetrazolium (NBT) (BIO-RAD Lab., Hercules, CA, USA) dissolved according to the manufacturer's instructions.
To a solution of 10-bromo-1-decanol (41 g, 0.17 mol, 1 equiv) in 130 mL of acetone at −5 °C was added slowly chromic acid solution prepared from CrO3 (25.7 g, 0.26 mol, 1.5 equiv), water (25 mL) and conc H2SO4 (22.5 mL, 0.34 mol, 2 equiv) at 0 °C, then stirred for 2 h and left over night at room temperature.
LC/MS Rt = 3.71 min. A solution of 6-bromo-3- naphthalen-2-yl -4- pyridin-4-yl pyridazine (7, 11.5 g, 32 mmol) in 95% ethanol (170 mL) was treated with 1-methylpiperazine (15.9 g, 158 mmol, 18 mL) and heated to reflux for 18 h.
Development of the blots was carried out with a solution of nitroblue tetrazolium/5-bromo-4-chloro-3-indolyl-phosphate (Roche).
To a solution of 2- 11-bromo-undecyl -isoindole-1,3-dione (1.53 g) in ethanol (55 ml), an aqueous solution of trimethylamine (Fluka, 45–50 %, 8.2- 11-bromo-undecyl -isoindole-1,3-dione
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